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The Malaysian Journal of Analytical Sciences, Vol 18 No 3 (2014): 629 - 641

629

THE EFFECTIVENESS OF POLYDIMETHYLSILOXANE (PDMS) AND

HEXAMETHYLDISILOXANE (HMDSO) AS COMPATIBILIZER ON THE

PREPARATION OF BETEL NUT FIBER (BNF) AND POLYPROPYLENE (PP)

/POLYSTYRENE (PS) WOOD COMPOSITES

(Keberkesanan Polidimetilsiloksana (PDMS) dan Heksametildisiloksana (HMDSO) Sebagai

Pengserasi Dalam Penyediaan Komposit Kayu Berasaskan Serabut Pinang dan Polipropilena

(PP)/Polistirena (PS))

Nurul Izzaty Khalid, Azizah Baharum*,Siti Sarah Ramli, Siti Norhana Mohd Nor

School of Chemical Science and Food Technology, Faculty of Science and Technology,

Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor, Malaysia.

*Corresponding author: [email protected]

Abstract

This research was carried out to investigate the effectiveness of polydimethylsiloxane (PDMS) and hexamethyldisiloxane

(HMDSO) as compatibilizing agent in producing wood composites of betel nut fiber/polypropylene (BNF/PP) and betel nut

fiber/polystyrene (BNF/PS). Wood composite was prepared by blending 40% of matrix polymer and 60% of treated and

untreated BNF using internal mixer Brabender Plasticoder at 170˚C with 50 rpm rotor speed for 13 minutes. The treatment was

done prior to blending the materials by immersing the BNF in PDMS and HMDSO solutions with 1%, 3% and 5% of

concentrations for 24 hours. The effects of 1% HMDSO treatment on BNF/PP composite contributed to high flexure strength and

impact strength which are 19.2 MPa and 7.9 kJ/M2 respectively while the percentage of water absorption showed the minimum

value of 6.7%. The impact strength of BNF/PS composite treated with 3% HMDSO showed maximum value that is 4.7 kJ/M2

and minimum percentage of water absorption, 6.8%. However, the flexure strength of untreated BNF/PS composite is higher

than treated BNF/PS composite with value of 4.7 MPa. The morphology of treated BNF/PP composites from SEM micrographs

showed better interface interaction between fibers and matrices. FTIR spectra showed the presence of siloxane groups such as Si-

O, Si-CH3, Si-(CH3) and Si(CH3) as a result of HMDSO and PDMS treatment. Based on the characterization analysis, HMDSO

treated composite of BNF/PP showed more effective interfacial interaction between BNF and matrices.

Keywords: polydimethylsiloxane, hexamethyldisiloxane, polypropylene, polystyrene, betel nut fiber, wood composite

Abstrak

Penyelidikan ini dijalankan untuk mengkaji keberkesanan polidimetilsiloksana (PDMS) dan heksadimetilsiloksana (HMDSO)

sebagai agen pengserasi dalam penghasilan komposit kayu berasaskan serabut pinang/polipropilena (SP/PP) dan serabut

pinang/polistirena (SP/PS). Komposit kayu disediakan dengan pengadunan 40% polimer matrik dan 60% SP terawat dan tak

terawat menggunakan mesin pengadun dalaman Brabender Plasticoder pada suhu 170˚C dengan kadar pengadunan 50 rpm

selama 13 minit. Rawatan ke atas SP dijalankan sebelum proses pengadunan dengan merendamkan SP selama 24 jam ke dalam

larutan PDMS dan HMDSO yang mempunyai peratus kepekatan berbeza iaitu 1%, 3% dan 5 %. Kesan daripada rawatan 1%

HMDSO ke atas komposit SP/PP telah menyumbang kepada peningkatan kekuatan lenturan dan hentaman dengan nilai masing-

masingnya ialah 19.2 MPa dan 7.9 kJ/M2, sementara peratus serapan air terhadap komposit ini menunjukkan nilai minimum iaitu

sebanyak 6.7%. Kekuatan hentaman bagi komposit SP/PS yang dirawat dengan 3% HMDSO menunjukkan nilai maksimum

sebanyak 4.7 kJ/M2 dan peratus serapan air yang minimum iaitu 6.8%. Walaubagaimanapun, kekuatan lenturan bagi komposit

SP/PS yang tak terawat lebih tinggi daripada komposit SP/PS yang terawat dengan bacaan kekuatan sebanyak 4.7 MPa.

Morfologi komposit SP/PP yang terawat dapat dilihat daripada mikrograf mikroskop imbasan elektron yang mana ia

menunjukkan interaksi antara muka yang lebih baik antara serabut dan matrik. Spektrum FTIR menunjukkan kehadiran

kumpulan siloksana seperti Si-O, Si-CH3, Si-(CH3) and Si(CH3) iaitu hasil daripada rawatan HMDSO dan PDMS. Berdasarkan

Nurul Izzaty et al: THE EFFECTIVENESS OF POLYDIMETHYLSILOXANE (PDMS) AND

HEXAMETHYLDISILOXANE (HMDSO) AS COMPATIBILIZER ON THE PREPARATION

OF BETEL NUT FIBER (BNF) AND POLYPROPYLENE (PP) /POLYSTYRENE (PS) WOOD

COMPOSITES

630

kepada analisis pencirian, komposit SP/PP yang dirawat dengan HMDSO menunjukkan interaksi antaramuka yang lebih

berkesan antara SP dan matriks.

Kata kunci: polidimetilsiloksana, heksametildisiloksana, polipropilena, polistirena, serabut pinang, komposit kayu

Introduction

Synthetic wood or wood composite is composite material produced from a mixture of plastic polymer and wood

flour or wood fiber [1]. It is designed widely due to certain factors such as environmentally friendly and do not

contribute to the waste of natural resources as most wood composite can be reprocessed [2]. The physical and

mechanical properties of wood composites have been found to possess toughness and stiffness, the strength of

stretching, resistance to impact and high resistance to weather where the properties are significantly important to

determine the product’s compatibility to be used in any applications [3-5]. The main components used in the

production of wood composite are natural fiber and matrix polymer. Natural fiber is dispersed phase and can be

categorized into three types, derived from animals, plants and minerals. Most of the natural fibers used in the

production of wood composite are from the plant such as blast sugarcane, kenaf and rice husk depends on the

suitability of a particular product to be produced.

In composite processing, increasing fiber composition potentially increases the mechanical properties of wood

composites [6-7]. Natural fiber replaces fiberglass used in many applications because it showed a significant

increase of the strength and flexibility as well as reduce weight composite products. Natural fiber used for this

research is betel nut fiber (Areca) which is mostly derived from renewable and biodegradable resources [8]. It can

be classified as short fiber as the average fiber length is in the range of 4 cm [9]. It contains certain components

comprising lignin (13 - 24.6%), hemicellulose (35 - 64.8%), ash content (4.4%) and water (8-25%) [10]. It

contained a large amount of very fine capillary found in the outer layer of fiber surface known as trichomes.

Trichomes are able to improve the adhesion of the interface between fiber and matrix polymer [11]. Thermoplastic

polymers used in this study are polypropylene (PP) and Polystyrene (PS), which is classified in group of

polyolefins. PP consist of propene monomer (C3H6) covalently bound to each other. PP is a semi-crystalline

polymer that will melt when heated and when frozen it will turn into a glassy state. PS (C8H8), is an aromatic

polymer made from the aromatic monomer of styrene. The melting point of PP is at a temperature of 160-175°C,

which allows it to be processed at a temperature lower than 200°C, a temperature that is used in the processing of

wood composite [12]. Polystyrene is an amorphous polymer in nature, brittle and rigid materials with its melting

point is at ~240°C. It is a thermoplastic material that is normally existed in a solid state at room temperature, melt

when heated at temperatures above 100°C and will return solid when cooled. Najafi et al [13] states that any plastic

or recycled plastic that can be melted and processed at temperatures below the degradation temperature of wood

filler can be used for production of wood composite.

Problems often arise when comes to the processing of wood composites using natural fibers and thermoplastic

matrix due to the different nature of fiber and matrix. Different nature of these two main components leads to

incompatibility at the fiber-matrix interphase and producing non-homogenous dispersion of fiber within the matrix.

Hydrophobic nature of the matrix has potential to protect the natural fiber from moisture. Therefore the fiber should

be evenly distributed throughout the matrix or coated with the polymer matrix completely to prevent moisture

absorption of composites produced [14]. Generally, additives or compatibilizing agent will increase compatibility

between hydrophilic wood and hydrophobic plastic and allows the formation of a single phase to occur [15]. Thus,

the siloxane group of polydimethylsiloxane (PDMS) and hexadimethylsiloxane (HMDSO) is used to modify the

surface of the fiber. PDMS is used as compatibilizer between natural fibers and thermoplastic matrix to improve the

physical and mechanical properties of wood composites and promote adhesion between two incompatible materials

[16]. According to Hocker [17], the treatment was conducted using HMDSO can make a material having a smooth

surface and a very high hydrophobicity effect of water contact angle.

The aim of this study was to investigate the effectiveness of polydimethylsiloxane (PDMS) and

hexamethyldisiloxane (HMDSO) as compatibilizing agent in producing wood composites of betel nut

fiber/polypropylene (BNF/PP) and betel nut fiber/polystyrene (BNF/PS).


631

Materials and Methods

Materials

The betel nut short fiber (BNF) used in this study was obtained from Faculty of Engineering and Built Environment,

Universiti Kebangsaan Malaysia (UKM). The matrices selected for this study were polypropylene (PP) and

polystyrene (PS) which was supplied by BDH Chemicals Ltd, Poole, England. The compatibilizing agent used was

polydimethylsiloxane (PDMS) with a density of 0.965 g/cm3

which was supplied by Acros Organics and

hexamethyldisiloxane (HMDSO) which was obtained from Sigma Aldrich, Steinheim, Germany. The isopropyl

alcohol used as solvent was supplied from Systerm, Shah Alam.

Preparation of Fiber

The BNF was prepared by separating the skin and its fruit. The layer of its skin was peeled to get the fiber and cut

into specific size within 0.5 – 1.0 cm. Then the fiber was dried under sunlight to remove moisture before being used.

PDMS and HMDSO Treatment

The treatment was carried out by immersing the dried fiber in PDMS and HMDSO solution with different

concentrations which were 1%, 3% and 5%, for about 24 hours at room temperature. The treated fiber were then left

in fume hood to let the solvent evaporate, rinsed several times with distilled water and finally dried in an oven at

104⁰C for 3 hours before being used.

Preparation of Wood Composite (BNF/PP and BNF/PS)

The untreated and treated BNF were blended with PP or PS using an internal mixer Brabender Plasticoder Model

PL 2000 with capacity of 60 cm3and composition ratio of fiber to matrix of 60:40. The blending was carried out at

170⁰C for about 13 minutes and mixing rate of 50 rpm. Then, the composites were compressed in mould with

hotpress machine to produce specimen with 3 mm thickness for further testing and analysis.

Fourier Transform Infra Red (FTIR) Analysis

The FTIR spectral analysis was done using Perkin Elmer Model BX machine at room temperature to determine the

functional group present in untreated and treated wood composite. The specimens with weight around 0.5 – 1 gram

were finely ground and mixed with potassium bromide (KBr) then pressed to form pellet for analysis.

Scanning Electron Microscope (SEM)

Scanning electron microscope (SEM) model LEO 1450VP were used to examine the morphology of untreated and

treated composites. Fractured specimen resulted from impact test were coated with gold in a hood Sputter model SC

500 to be analyzed. The scanning electron micrographs were then studied to define the fiber-matrix interphase

before and after treatment.

Impact Test

Unnotched Izod impact test were tested using a Digital Pendulum Machine model RR/MT (Ray Ran) with a 2.706 J

pendulum. Eight specimens were cut into 65 mm x 12 mm x 3 mm according to ASTM D 4812 and the best five

results were calculated to get an average impact value.

Flexural Test

Flexural tests were performed using universal testing machine (Instron model 5567) according to ASTM D 790.

Three point bending method with load cell 10 kN and speed of 1.3 mm/min were done on five duplicated samples,

with dimensions of 120 mm x 12 mm x 3 mm, to determine average flexural value.

Water Absorption Test

This test was conducted according to ASTM D 570 to determine the total water absorption by two duplicated

samples for each composite in 24 hours. The specimens were oven dried at 104 ˚C for 2 hours prior to testing and

then were put into desiccators to avoid moisture during cooling process. The weight of dry sample was taken before

and after immersing the samples in 200 mL of water for 24 hours. Total of water uptake were determined using the

following equation (1):




COMPOSITES

632

Mt(%) = 100XW

WW

o

ot (1)

where,

Mt = Total water uptake at time t

Wt = Weight of sample at time t

Wo = Weight before immersion

Results and Discussion

Flexural Test

Flexural modulus is determined to know the stiffness of composite towards flexure. To analyze the data, each data

represented treated composites compared to the untreated composites. Figure 1 shows better flexural modulus for

BNF/PP composites treated with HMDSO where 1% HMDSO is the optimum concentration which gives a rise to

24.2% increment. Meanwhile the flexural modulus decreased around 9.9% and 30.3% for BNF/PP treated with 3%

and 5% HMDSO respectively. This result reveals that only a small portion of compatibilizer needed to trigger an

effective interphase reaction and improved the homogeneity of fiber and matrix. The concept can be applied to the

use of PDMS compatibilizer where 1% PDMS led to an increase of 16.7% in flexural modulus. Even though PDMS

contained the same functional group as HMDSO and acted as compatibilizer, the flexural modulus for BNF/PP

treated with 3% and 5% PDMS is reduced due to agglomeration and entanglement of longer PDMS chain in treated

fiber.

Figure 1. The effect of PDMS and HMDSO treatments with a series of concentration on the flexural modulus of

BNF/PP and BNF/PS wood composites

2511 2931

2076

1430

3118

2263

1751

6406

4207 3846

4198 4095

4930

3476

0

1000

2000

3000

4000

5000

6000

7000

untreated 1% PDMS 3% PDMS 5% PDMS 1%

HMDSO

3%

HMDSO

5%

HMDSO

Fle

xura

l M

od

ulu

s (M

Pa)

Composites

BNF/PP

BNF/PS


633

Flexural strength of BNF/PP containing PDMS as compatibilizing agent for all concentrations is lower than

untreated composites as shown in Figure 2. However, the flexural strength of BNF/PP treated with HMDSO at all

testing concentrations depicts better reading than the untreated composites. The BNF/PP composites treated with

1% HMDSO increased the flexural strength by 18.5%. Based on the trend of flexural modulus and flexural strength

of BNF/PP composites, it can be concluded that the modulus is proportional to flexural strength for both types of

treatment. The trend shows decrement as the percentage of compatibilizer concentration increased.

As can be seen in Figure 1, the flexural modulus of untreated BNF/PS is much higher than untreated BNF/PP.

However, the BNF/PS treated with PDMS and HMDSO both has reduced the flexural modulus around 35.6%. The

trend also goes similarly with flexural strength of BNF/PS treated with PDMS and HMDSO with decrement around

41.7%. Untreated BNF has many small furry spaces which known as trichomes that stand out of fiber surface. The

increment in the flexural result of untreated BNF/PS might be due to effective interaction between trichomes and PS

matrices. After treatment, thin layer of PDMS and HMDSO that formed on surface of BNF in BNF/PS composite

might reduce the interaction between trichomes and the PS matrices (Figure 9 (e) and (f)).

In particular, this research found that flexural strength of BNF/PP composites treated with HMDSO is higher than

composites treated with PDMS while both HMDSO and PDMS treatments did not improved flexural properties of

BNF/PS composites.

Figure 2. The effect of PDMS and HMDSO treatments with a series of concentration on the flexural strength of


Impact Test

Figure 3 shows impact strength of composites. The impact strength of BNF/PP shows increment after treatment

with PDMS but the impact strength decreased with the increase of concentration of HMDSO. BNF/PP with 1%

HMDSO treatment has the highest impact strength with an increase at 70.3% compared to other treated composites.

The higher the impact strength leads to higher rigidity of composite. Thus it requires high kinetic energy during

16.2 14.6 14.3

10.5

19.2 18.3 17.8

46.2

23.5 22.1

28.3 26.9

37.4

23.6

0

5

10

15

20

25

30

35

40

45

50


HMDSO

3%

HMDSO

5%

HMDSO

Fle

xura

l s

tren

gth

(M

Pa)

Composites

BNF/PP

BNF/PS




COMPOSITES

634

impact to initiate crack propagation until it breaks. The increase of impact strength for BNF/PP treated with

increasing concentration of PDMS is due to the addition of long chain of PDMS which absorbed impact strength

effectively. Weak interfacial interaction leads to the formation of micro spaces between fiber and matrix. When an

impact is applied on samples, micro fracture will occur and lead to crack dispersion. As a result, the impact strength

needed to fracture the sample is lower.

PS matrix in crystalline form exhibits low impact energy. As shown in Figure 3, BNF/PS treated with 3% of

HMDSO increased the impact strength by 38.2%, more than other treated and untreated BNF/PS. This improvement

could be related to flexible Si-O-Si chains from the compatibilizer. HMDSO and PDMS treatment on fiber

improved the compatibility between fiber and matrix because it allows a better load transfer from matrix to fiber

during impact due to strong bond of fiber-matrix.

Figure 3. The effect of HMDSO and PDMS treatment with a series of concentration on the impact strength of


Water Absorption Test

Generally, water absorption of treated BNF/PP composite shows lower value than untreated composite as proven in

Figure 4. Main components in fiber such as hemicelluloses, cellulose and lignin are able to absorb water and

moisture from environment. Based on past research by Agnantopoulou et al [18], they found that hemicelluloses is

more hygroscopic element as it contains more hydroxyl group than lignin. The hollow cavity which known as

lumen formed from fiber cell units are also available to generate more space or passage for water to seep into the

fiber. Therefore, the treatment caused wood composite to become less hygroscopic due to the distribution and

dispersion of compatibilizer which fulfill the wood cell wall space, in turn exhibiting hydrophobic properties.

Diffusion of water and other molecules in the cell walls was also reduced because the compatibilizer has blocked

micropores in the cell walls which resulting hygroscopic properties of wood composites to decrease.

4.64

5.18 5.24

6.09

7.9

6.55

5.6

3.4

3.9

2.7

4.2 4.1

4.7

2

0

1

2

3

4

5

6

7

8

9


HMDSO

3%

HMDSO

5%

HMDSO

Imp

act

Str

ength

(kJ/

M2)

Composites

BNF/PP

BNF/PS


635

However, the trend for BNF/PS composite is different with BNF/PP composite where only 3% HMDSO treatment

showed improvement on water resistivity by an increment around 11.7%. The other treated BNF/PS composite

shows higher water absorption than untreated composite probably due to poor fiber–matrix interaction in the

composite. Additives treatment has possibility to increase or to decrease the percentage of water absorption as stated

by Gnatowski [19].The treatment with 1% HMDSO on BNF/PP composite has decreased the percentage of water

absorption by 61.9% due to the formation of hydrophobic layer on the fiber surface. HMDSO posses strong water

resistivity to block water diffusion into voids of fiber. HMDSO treatment results in the smooth surface of fiber.

Figure 4. The effect of HMDSO and PDMS treatment with a series of concentration on the water absorption by


FTIR Spectra Analysis

The FTIR spectral analysis of untreated and treated composites is shown in Table 1. For both untreated BNF/PP and

BNF/PS, there were peaks at 3663 cm-1

and 3433 cm-1

respectively due to hydroxyl group (OH) of cellulose in

fiber. In addition, other peaks were also present which belong to CH stretch, carbonyl (CO) and ether (C-O-C)

groups in both untreated composites. Based on the spectrum of BNF/PP treated with HMDSO in Figure 6, OH and

C-H stretching from cellulose fiber can be observed at 3305 cm-1

and 2754 cm-1

respectively. There were no peak

presence for ether group from cellulose and lignin because of impurities such as dust or water molecule since it can

resist the absorption of any peak on spectrum. PP matrix is identified at 2874cm-1

for bent CH3 group. FTIR

spectrum of treated composites from both PP and PS showed several peaks at 785 cm-1

, 846 cm-1

and 1202 cm-1

which attributed to Si(CH3), Si-C stretching vibration and Si-O stretching respectively that occur due to the physical

interaction of fiber and HMDSO. Theoretically, HMDSO formed a thin layer on the surface of fiber without

experiencing any chemical reaction to form new chain. The presence of Si-O-Si chains in HMDSO structure with

elasticity properties gives high flexibility in composites by increasing the flexural strength as shown by the flexural

test results.

17.6

9.4

11.8 12.6

6.7

13.4

9.5

7.7

13.5 12.6

8.5

14.3

6.8

16.5

0

2

4

6

8

10

12

14

16

18

20


HMDSO

3%

HMDSO

5%

HMDSO

Per

centa

ge

of

Wat

er A

bso

rpti

on (

%)

Composites

BNF/PP

BNF/PS




COMPOSITES

636

Table 1. FTIR analysis of untreated and HMDSO treated composite

Functional Group Wavenumbers, cm-1

Untreated

BNF/PP

HMDSO treated

BNF/PP

Untreated

BNF/PS

HMDSO treated

BNF/PS

OH 3663 3305 3433 3525

CH 2983 2754 2917 2920

CO 1060 - 1044 1035

C-O-C 1146 - 1149 1123

CH3 (symmetry and

asymmetry) 2983 - - -

CH3 (bent) - 2874 - -

C-H (aromatic

stretching) - - 3433 3060

Si(CH3)- - 785 - 746

Si-C (vibration

stretching at Si-CH3

and Si(CH3)-)

- 846 - 844

Si-O (stretching) - 1202 - 1071

Figure 5. FTIR spectrum of untreated BNF/PP composite


637

Figure 6. FTIR spectrum of BNF/PP treated with HMDSO

Figure 7. FTIR spectrum of untreated BNF/PS composite




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Figure 8. FTIR spectrum of BNF/PS treated with HMDSO

Scanning Electron Microghraphs

SEM micrograph from Figure 9(a) showed the presence of microvoids for untreated BNF/PP composite which

mostly covered by trichomes as it is a major component in BNF. PP matrix can be seen binding at a random

position due to the variation of fiber size from 0.5 – 1.0 cm. Besides, it is found that fiber pulled out occurred in the

specimen because of weak adhesion interaction at fiber-matrix interphase. After 1% HMDSO treatment on BNF/PP

composites, the HMDSO coated most of the trichomes on the fiber. Adhesion between treated BNF and PP matrix

was found to be more compatible and showed fiber breakage at the fractured surface as in Figure 9(b) because of

better interface and interphase interaction in the composite However, for 1% PDMS in the BNF/PP composite, both

fiber pulled out and fiber breakage could be seen on the fractured surface compare to 1% HMDSO treated BNF/PP

composite (Figure 9(c)).

Based on Figure 9(d), it is observed that BNF were tightly interacted within PS matrix due to trichomes on the

surface of BNF, provides better adhesion of fiber–matrix interface which supported the flexural strength data of

untreated BNF/PS in Figure 2. SEM micrographs from Figure 9(e) and 9(f) clearly show that, the fractured surface

exhibited many voids as the fiber was pulled out from PS matrix after impact test. Treatment with 3% HMDSO

provides better compatibility at fiber-matrix interphase than treatment with 3% PDMS and it resulted in fewer voids

after the treatment. However, treated BNF/PS only increases the impact strength and water absorption.


639

Figure 9. SEM micrographs of composites with magnification of 300x: (a) Untreated BNF/PP, (b) BNF/PP with 1%

HMDSO, (c) BNF/PP with 1% PDMS, (d) Untreated BNF/PS, (e) BNF/PS with 3% HMDSO, (f) BNF/PS

with 3% PDMS

(a) (b)

(c) (d)

(e) (f)




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640

Conclusion

The effects of the HMDSO and PDMS treatments on the BNF/PP and BNF/PS were investigated in this study.

Generally, treatment with HMDSO was better than PDMS and show that HMDSO acted better as compatibilizing

agent in BNF/PP composite. This is due to simple structure of HMDSO resulting in homogeneity between fiber and

matrices. SEM micrograph also revealed that the microvoids of BNF/PP and BNF/PS was reduced after HMDSO

treatment and it is proved by FTIR spectral analysis which indicate peaks Si(CH3), Si-C stretching vibration and Si-

O stretching that show physical interaction at fiber-matrix interphase. The results revealed 1% HMDSO as the

optimum amount to be used as compatibilizer for BNF/PP composite where the compatibility of fiber-matrix

interphase was significantly improved and contributed to the increment of flexural strength (18.5%), flexural

modulus (24.2%), impact strength (70.3%) and percentage of water absorption (61.9%). PDMS and HMDSO are

not effective as compatibilizers in BNF/PS composite and showed no significant improvement on their mechanical

properties.

Acknowledgement

The authors would like to thank the Department of Chemistry, Faculty of Science and Technology, National

University of Malaysia and lab technicians for the technical support of this project.

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